CN1029112C - Method for extracting alkali metal compound from lepidolite concentrate - Google Patents
Method for extracting alkali metal compound from lepidolite concentrate Download PDFInfo
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- CN1029112C CN1029112C CN 92106977 CN92106977A CN1029112C CN 1029112 C CN1029112 C CN 1029112C CN 92106977 CN92106977 CN 92106977 CN 92106977 A CN92106977 A CN 92106977A CN 1029112 C CN1029112 C CN 1029112C
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- Prior art keywords
- roasting
- stripping
- lime
- lithium
- quilonum retard
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000012141 concentrate Substances 0.000 title claims abstract description 16
- 150000001339 alkali metal compounds Chemical class 0.000 title claims description 3
- 229910052629 lepidolite Inorganic materials 0.000 title abstract 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 21
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 18
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 17
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 10
- 239000011591 potassium Substances 0.000 claims abstract description 10
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims abstract description 9
- 229910052701 rubidium Inorganic materials 0.000 claims abstract description 8
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000011084 recovery Methods 0.000 claims abstract description 7
- 235000017550 sodium carbonate Nutrition 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 14
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 14
- 239000004571 lime Substances 0.000 claims description 14
- 239000012452 mother liquor Substances 0.000 claims description 10
- 230000008020 evaporation Effects 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 239000004411 aluminium Substances 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000004513 sizing Methods 0.000 claims description 5
- -1 Cesium compound Chemical class 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 3
- 235000015320 potassium carbonate Nutrition 0.000 claims description 3
- 230000002000 scavenging effect Effects 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 238000005342 ion exchange Methods 0.000 claims description 2
- 239000012047 saturated solution Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims 3
- 239000001569 carbon dioxide Substances 0.000 claims 1
- 229910002092 carbon dioxide Inorganic materials 0.000 claims 1
- 235000011089 carbon dioxide Nutrition 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 150000003112 potassium compounds Chemical class 0.000 claims 1
- 238000000746 purification Methods 0.000 claims 1
- 150000003388 sodium compounds Chemical class 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052808 lithium carbonate Inorganic materials 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 239000003513 alkali Substances 0.000 abstract description 4
- 238000010411 cooking Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000000227 grinding Methods 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 abstract 1
- 239000000292 calcium oxide Substances 0.000 abstract 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000012768 molten material Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 235000011121 sodium hydroxide Nutrition 0.000 description 8
- 239000002585 base Substances 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910052728 basic metal Inorganic materials 0.000 description 3
- 150000003818 basic metals Chemical class 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 239000006028 limestone Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- HQRPHMAXFVUBJX-UHFFFAOYSA-M lithium;hydrogen carbonate Chemical compound [Li+].OC([O-])=O HQRPHMAXFVUBJX-UHFFFAOYSA-M 0.000 description 2
- 239000010445 mica Substances 0.000 description 2
- 229910052618 mica group Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910000024 caesium carbonate Inorganic materials 0.000 description 1
- 239000000404 calcium aluminium silicate Substances 0.000 description 1
- 235000012215 calcium aluminium silicate Nutrition 0.000 description 1
- WNCYAPRTYDMSFP-UHFFFAOYSA-N calcium aluminosilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O WNCYAPRTYDMSFP-UHFFFAOYSA-N 0.000 description 1
- 229940078583 calcium aluminosilicate Drugs 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- HOOWDPSAHIOHCC-UHFFFAOYSA-N dialuminum tricalcium oxygen(2-) Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[Al+3].[Al+3].[Ca++].[Ca++].[Ca++] HOOWDPSAHIOHCC-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- ZLMJMSJWJFRBEC-OUBTZVSYSA-N potassium-40 Chemical compound [40K] ZLMJMSJWJFRBEC-OUBTZVSYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- IGLNJRXAVVLDKE-IGMARMGPSA-N rubidium-85 atom Chemical compound [85Rb] IGLNJRXAVVLDKE-IGMARMGPSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/06—Preparation via sodium or potassium magnesium carbonate
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A pressure cooking method for preparing lithium carbonate from lepidolite ore concentrate includes such steps as introducing steam to ore concentrate for calcining, adding mixed alkali (calcium oxide, sodium carbonate or sodium hydroxide) to the molten material, grinding, regulating size, purifying solution, evaporating for concentrating, extracting lithium by carbonation, recovering mixed alkali, and recovering potassium, rubidium and caesium. The invention has the characteristics of low pressure and temperature in the dissolving-out process, simple production process, easy solution of production equipment, safe and reliable operation, low energy consumption, small alkali consumption (only 0.6 ton of sodium carbonate is consumed by each ton of lithium carbonate), low production cost, high metal recovery rate and the like, and can be popularized and applied in industrial production.
Description
The present invention relates to a kind of lithionite concentrate and make the method that raw material comprehensively extracts alkali metal compound.
Generally contain alkalimetal oxides such as lithium, sodium, potassium, rubidium, caesium in the lithionite ore deposit.In the extraction metallurgy of lithionite, R.B.Norden(Chcm.Eng.1956.3p288～291 in 1956) lithionite-limestone sintering method manufacture order water lithium hydroxide is disclosed.It is to be that 3～4 proportioning is mixed by weight with Wingdale and lithionite, and wet-milling to granularity is to send in the rotary kiln after 0.074 millimeter, is to carry out roasting under 875～911 ℃ in temperature.Carry out two sections strippings after the shrend of roasting material chilling, levigate (0.074 millimeter of the granularity).Dissolution fluid adds milk of lime and removes aluminium, and condensing crystal makes the monohydrate lithium hydroxide product.1979, C.A.Olivier etc. (CIM Bulletin, 1979, Vol.72, NO.807, P.131～136) disclosed yellow soda ash and have pressed cooking method to produce the test-results of Quilonum Retard continuously.This method is with the β-triphane after levigate (0.074 millimeter of granularity), by sodium/lithium (atom) than being 1.15 to allocate into and return mother liquor and yellow soda ash, the slip that furnishing contains solid 30% is continuously pumped into is with churned mechanically autoclave, keeping the still temperature with electric heating is 200～220 ℃, after reaction is finished, through three grades of relievers and cooling system discharging, cooling, when being cooled to 20 ℃, the stripping slurries feed CO
2Make Quilonum Retard change the bigger lithium bicarbonate of solubleness into, press filtration separates the solution behind the residue, makes heating medium with glycol, makes the lithium bicarbonate thermolysis make the product Quilonum Retard.Preceding a kind of limestone sintering method, raw material sources are extensive, and are cheap, yet exist mass flow big, plant efficiency is low, the energy consumption height, shortcomings such as metal recovery rate is low, a kind of yellow soda ash in back is pressed cooking method, and only needing yellow soda ash is solvent, a small amount of caustic soda is used for mother liquor regeneration, product Quilonum Retard purity height, the stripping slag can fully utilize, and does not have corrosion, but stripping temperature height needs high-tension apparatus and CO
2Regeneration system rapidly, thereby production cost height.
The present invention is directed to the problem that aforesaid method exists, propose a kind of low-temp low-pressure mixed base and press cooking method to produce Quilonum Retard, can make major metal rate of recovery height, the extraction metallurgical method that other valuable metal is comprehensively reclaimed.
Technical scheme of the present invention is: the roasting of lithionite concentrate, and levigate the sizing mixing of preparing burden pressed and boiled stripping, and dissolution fluid removes aluminium and purifies, evaporation concentration, the carbonic acid ratio is carried lithium, and evaporation concentration is carried sodium, reclaims byproduct potassium chemical combination and rubidium, Cesium compound.
Further embodiment of the present invention, be that lithionite concentrate (＜0.18 millimeter) is placed rotary kiln, fed steam roasting 10～40 minutes down at 870～930 ℃, make that most of fluorine is removed in the concentrate, variation has taken place in mineral structure simultaneously, obtain the roasting material of the loose porous easy mill of grey black, add mixed base (as lime by certain weight ratio then, yellow soda ash or sodium hydroxide) carry out ground and mixed, add the water batching of sizing mixing, for example according to roasting material, lime, the weight ratio of yellow soda ash (or sodium hydroxide) is 10: (3～10): (1～6), liquid-solid ratio is 4～6, place the autoclave stripping with above-mentioned through the ground and mixed slip, boiling temperature when pressure is 120～150 ℃, and pressure is (2～5) * 10
5Handkerchief, dissolution time are that the basic metal solubility rate is (%): lithium 92～96, potassium 40～90, rubidium 85, caesium 40 under 2～4 hours the condition; In process in leaching, Al
2O
3, SiO
2, F also has and follows basic metal to be dissolved together on a small quantity, so the stripping slurries after filtration the filtrate behind the deslagging need add lime, make the Al in the solution
2O
3, SiO
2, impurity such as F generates the very little tricalcium aluminate (3CaOAl of solubleness respectively
2O
310H
2O), calcium aluminosilicate hydrate (3CaOAl
2O
3XSiO
2YH
2O) and Calcium Fluoride (Fluorspan) (CaF
2) precipitate and separate out, with this cleansing soln.When lime interpolation excess coefficient is 2～4, at room temperature stirred 2～4 hours, to remove aluminium efficient and reach 99%, silica removal efficient reaches 90%, and fluorine-based eliminates, and the loss of basic metal in removing the aluminium scavenging process is less than 5/1000ths.
Scavenging solution after the removal of impurity at first carries out evaporation concentration, till solution concentration to sodium hydroxide is not separated out with yellow soda ash when the carbonating, then feeds limestone kiln tail gas (CO
2) make alkali metal hydroxide change alkaline carbonate into, this procedure generally is referred to as carbonating.Because the solubleness of alkaline carbonate is pressed Li under comparatively high temps
2CO
3→ Na
2CO
3→ K
2CO
3→ Rb
2CO
3→ Cs
2CO
3Order increase, the solubleness minimum (0.72 gram/100 gram water, 100 ℃) of Quilonum Retard in water, and reduce along with the rising of other carbonate concentration, also Quilonum Retard and other carbonate do not generate double salt and complex salt, so Li in the carbonation
2CO
3Preferential crystallization is separated out, and other alkaline carbonate is still stayed (all the end reaches its saturation concentration) in the solution.The Quilonum Retard filtered while hot that crystallization is separated out is separated, and stirs wash clean with the Quilonum Retard saturated solution then; Washing lotion is returned evaporation concentration, and crystallization Quilonum Retard drying makes the Li that meets Chinese Industrial Standards (CIS) GB11075-89 specification of quality
2CO
3The Quilonum Retard output capacity can reach 90%.
Carbonating is put forward the further evaporation concentration of mother liquor behind the lithium, and crystallize sodium carbonate is separated out, and facts have proved that its eduction rate can reach 90%.The yellow soda ash of being separated out can directly return batching, or adds lime causticization and obtain sodium hydroxide and return batching again, recycles.Therefore, lithium carbonate product per ton only consumes the yellow soda ash about 0.6 ton.Carry the mother liquor behind the sodium, feed CO
2Carry out second time carbonating and obtain saleratus, adopt the method for recrystallization to improve its grade, obtain byproduct salt of wormwood after the roasting.The mother liquor of carrying after the signature reclaims rubidium, Cesium compound with extraction process or ion exchange method; Perhaps preserve, handle again after treating as the form of rubidium, caesium blended solid alkali.
The present invention compares with documents 1, has following advantage: the material handling amount is few in (one) technical process, in roasting, clinker grinding mill spy industry be its 1/4th, in the stripping operation be its 1/2nd; (2) metal recovery rate height, the solubility rate of lithium is (%) 92～96, comprehensive utilization is made good use of; (3) total energy consumption is low, can save lot of energy; (4) production cost is low, and is good in economic efficiency; (5) waste gas, waste water can reach discharging standards after treatment.
Fig. 1 is pressurized boiling process for preparing lithium carbonate with lithium mica ore and mixed base and comprehensively recovering valuable metal compound schema.
Provide the following example replenishing in conjunction with Fig. 1 and certain lithionite ore deposit as embodiment of the present invention.The chemical ingredients of China's somewhere lithionite concentrate is (%): Li
2O4.56, Na
2O1.20, K
2O8.60, Rb
2O1.40, Cs
2O
30.29, Al
2O
324,02, SiO
252.67, Fe
2O
30.36, CaO0.15, MgO0.01, MnO0.20, F5.68.
Example 1. with the lithionite concentrate (＜0.18mm) fed steam roastings 25 minutes down, as stripping roasting material 890 ℃ of temperature.When roasting material 10 grams, allocate lime 6 grams into, sodium hydroxide 5 grams add 70 milliliters in clear water, at 130 ℃ of temperature, pressure 2.8 * 10
5Under the handkerchief condition, press and boiled stripping 3 hours, the solubility rate 91.36% of lithium, the solubility rate 92.07% of potassium, the solubility rate 89.0% of rubidium, the solubility rate 38.71% of caesium.
Example 2. with the lithionite concentrate (＜0.18mm) fed steam roastings 25 minutes down, as stripping roasting material 890 ℃ of temperature.When roasting material 10 grams, allocate lime 6.8 grams into, sodium hydroxide 2 grams add 70 milliliters in clear water, boil stripping 3 hours 140 ℃ of temperatures, the solubility rate 92.53% of lithium, the solubility rate 80.68% of potassium.
Example 3. with the lithionite concentrate (＜0.18mm) fed steam roastings 25 minutes down, as stripping roasting material 890 ℃ of temperature.When roasting material 10 grams, allocate lime 4.5 grams into, yellow soda ash 4 grams add 80 milliliters in clear water, boil stripping 3 hours 130 ℃ of temperatures, the solubility rate 92.05% of lithium, the solubility rate 43.13% of potassium.
Example 4. with the lithionite concentrate (＜0.18mm) fed steam roastings 25 minutes down, as stripping roasting material 875 ℃ of temperature.When roasting material 10 grams, allocate lime 6.8 grams into, sodium hydroxide 5 grams add 70 milliliters in clear water, boil stripping 3 hours 150 ℃ of temperatures, the solubility rate 94.54% of lithium, the solubility rate 83.52% of potassium.
Example 5. with the lithionite concentrate (＜0.18mm) fed steam roastings 20 minutes down, as stripping roasting material 880 ℃ of temperature.When roasting material 10 grams, allocate lime 3 grams into, yellow soda ash 4 grams add 70 milliliters in clear water, press down for 130 ℃ in temperature and boil stripping 3 hours, the solubility rate 91.53% of lithium, the solubility rate 64.77% of potassium.
With the dissolution fluid of above-mentioned example 1,2,3,4,5 gained through remove aluminium and purify and evaporation concentration after, feed CO
2Carry out carbonating and carry lithium, after filtration, washing, oven dry obtain meeting the Quilonum Retard of Chinese Industrial Standards (CIS) GB11075-89 specification of quality.Lithium liquor continuation evaporation is separated out yellow soda ash and is returned the batching of sizing mixing, and perhaps returns batching again through causticization; Analyse behind the sodium mother liquor once more carbonating obtain saleratus, will make byproduct salt of wormwood after its roasting again; Mother liquor adopts extraction process to separate after carrying potassium, obtains rubidium, caesium carbonate.
Claims (1)
1, a kind of method from lithionite concentrate extraction alkali metal compound, this method may further comprise the steps: the roasting of lithionite concentrate, stripping, dissolution fluid add lime and remove aluminium purification, condensing crystal, it is characterized in that:
(1) roasting is that the lithionite concentrate is placed 870～930 ℃ high temperature and fed steam roasting 10～40 minutes;
(2) stripping, be that weight ratio by roasting material, lime, yellow soda ash (or sodium hydroxide) is 10: (3～10): (1～6), liquid-solid ratio is 4～6 to carry out mix, and mixing section is ground size mixing that to be placed on temperature be that 120～150 ℃, pressure are (2～5) * 10
5Press in the autoclave of handkerchief and boiled 2～4 hours;
(3) removing aluminium and purify, is with the stripping slurries filtrate behind the deslagging after filtration, adds excess coefficient and be 2～4 lime, at room temperature stirs 2～4 hours;
(4) carbonating system Quilonum Retard, be when the scavenging solution evaporation concentration is not extremely separated out sodium hydroxide as yet, feed carbon dioxide and carry out carbonating, alkali metal hydroxide is converted into alkaline carbonate, with its separately the different solubility preferential crystallization separate out Quilonum Retard, filter and make the product Quilonum Retard through the washing of Quilonum Retard saturated solution, oven dry;
(5) recovery of sodium compound is to continue evaporative crystallization and separate out yellow soda ash and directly return the batching of sizing mixing carrying mother liquor behind the lithium, and the yellow soda ash of perhaps separating out adds lime causticization and makes sodium hydroxide and return the batching of sizing mixing;
(6) recovery of potassium compound, be with carry mother liquor behind the sodium feed carbonic acid gas once more carbonating obtain saleratus, make product salt of wormwood through roasting;
(recovery of 7) Jia, Cesium compound is that the mother liquor that will carry behind the potassium adopts extraction process or ion exchange method to extract rubidium, Cesium compound respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106977 CN1029112C (en) | 1992-06-23 | 1992-06-23 | Method for extracting alkali metal compound from lepidolite concentrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106977 CN1029112C (en) | 1992-06-23 | 1992-06-23 | Method for extracting alkali metal compound from lepidolite concentrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1067028A CN1067028A (en) | 1992-12-16 |
| CN1029112C true CN1029112C (en) | 1995-06-28 |
Family
ID=4942596
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92106977 Expired - Fee Related CN1029112C (en) | 1992-06-23 | 1992-06-23 | Method for extracting alkali metal compound from lepidolite concentrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1029112C (en) |
Cited By (1)
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| WO2024002486A1 (en) * | 2022-06-30 | 2024-01-04 | Lülsdorf Functional Solutions Gmbh | Improved process for the preparation of potassium hydrogencarbonate |
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| CN111268705B (en) * | 2020-03-06 | 2021-05-25 | 中国地质大学（北京） | Method for preparing lithium carbonate by using lepidolite powder |
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1992
- 1992-06-23 CN CN 92106977 patent/CN1029112C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024002486A1 (en) * | 2022-06-30 | 2024-01-04 | Lülsdorf Functional Solutions Gmbh | Improved process for the preparation of potassium hydrogencarbonate |
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| CN1067028A (en) | 1992-12-16 |
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